反应 #5023

ord-fa8c1a5973204abeab956b536c71aec8

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度to refluxing for 5 hours with vigorous stirring
  2. 2
    过滤The reaction mixture was filtered by suction while hot
  3. 3
    其他to remove insoluble matter
  4. 4
    浓缩the filtrate thereof was concentrated
  5. 5
    温度cooled

实验过程

To a mixed solution of ethanol (400 ml) and water (100 ml), were added N-acetyl-5-bromo-7-nitroindoline (133.1 g), iron powder (10 mesh; 75 g) and concentrated hydrochloric acid (5 ml), and the mixture was subjected to refluxing for 5 hours with vigorous stirring. The reaction mixture was filtered by suction while hot to remove insoluble matter, and then the filtrate thereof was concentrated and cooled on standing to give the intended compound 38.3 g (32.2%) as a brown needle crystal. M.P.: 154°-155° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05242912uspto-grants-1993_09